CN115067358B - Ag/Zn ion loaded black titanium dioxide composite molybdenum disulfide nanosheet nanomaterial - Google Patents
Ag/Zn ion loaded black titanium dioxide composite molybdenum disulfide nanosheet nanomaterial Download PDFInfo
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- CN115067358B CN115067358B CN202210703908.3A CN202210703908A CN115067358B CN 115067358 B CN115067358 B CN 115067358B CN 202210703908 A CN202210703908 A CN 202210703908A CN 115067358 B CN115067358 B CN 115067358B
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 52
- 150000002500 ions Chemical class 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000002135 nanosheet Substances 0.000 title claims abstract description 31
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 40
- 239000004408 titanium dioxide Substances 0.000 title claims description 20
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 36
- 239000011701 zinc Substances 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 229910052709 silver Inorganic materials 0.000 claims abstract description 18
- 239000004332 silver Substances 0.000 claims abstract description 18
- 229920001661 Chitosan Polymers 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000001699 photocatalysis Effects 0.000 abstract description 20
- 230000001954 sterilising effect Effects 0.000 abstract description 18
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 10
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 description 15
- 230000000694 effects Effects 0.000 description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- 230000002147 killing effect Effects 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- 230000004298 light response Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- -1 silver ions Chemical class 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000003384 imaging method Methods 0.000 description 3
- 239000002064 nanoplatelet Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000004627 transmission electron microscopy Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
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- 238000011065 in-situ storage Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- AHVYPIQETPWLSZ-UHFFFAOYSA-N N-methyl-pyrrolidine Natural products CN1CC=CC1 AHVYPIQETPWLSZ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001599 direct drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000002555 ionophore Substances 0.000 description 1
- 230000000236 ionophoric effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- BSWGGJHLVUUXTL-UHFFFAOYSA-N silver zinc Chemical compound [Zn].[Ag] BSWGGJHLVUUXTL-UHFFFAOYSA-N 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
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Abstract
The invention belongs to the technical field of photocatalysis sterilization materials, and relates to Ag/Zn ion-loaded black TiO 2 Composite MoS 2 A nano-sheet nano-material and a preparation method thereof. The preparation method comprises the following steps: (1) Mixing molybdenum disulfide, chitosan, nano titanium dioxide and an organic solvent to obtain a mixed solution; (2) Ball milling is carried out on the mixed solution, and then heating and drying are carried out to obtain a powder sample; (3) Mixing the powder sample with NaBH 4 Mixing and grinding the powder, then placing the powder into a tube furnace for heat treatment for a period of time, and introducing Ar gas for protection; (4) Dispersing the mixed powder obtained by the heat treatment in deionized water for ultrasonic treatment, adding salt containing silver/zinc ions under stirring, and drying to obtain the nano material. The preparation method of the invention has the advantages of simple and convenient operation, easy realization, low consumption, high yield, good repeatability, suitability for large-scale production and no secondary pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of photocatalysis sterilization materials, and relates to Ag/Zn ion-loaded black TiO 2 Composite MoS 2 A nano-sheet nano-material and a preparation method thereof.
Background
The photocatalysis technology is a technology for efficiently solving the environmental pollution and improving public health. Titanium dioxide (TiO) 2 ) Is a stable and cheap high-efficiency inorganic photocatalytic material, and due to the advantages of high photocatalytic performance, high stability, low toxicity, low price, environmental protection and the like, the TiO 2 Can generate photocatalysis reaction under the excitation of ultraviolet rays, and finally decompose organic matters into carbon dioxide and water. Thus, tiO 2 The photocatalytic material can be used in the fields of organic matter removal, sterilization, disinfection, sewage treatment and the like.
However, only 4-5% of the UV component of sunlight greatly limits TiO 2 Is used for photocatalytic applications. To better realize TiO 2 The solar light response can be realized by modifying means such as metal/nonmetal ion doping, noble metal loading, structure heterojunction semiconductor and the like. Wherein, the heterojunction structure can be effectively improved by constructing the heterojunction structure with other semiconductor nano-materials 2 Is a cheap and environment-friendly process. And as a graphene-like two-dimensional semiconductor nanomaterial, few-layer molybdenum disulfide (MoS 2 ) The unique band gap structure of the nano sheet enables the nano sheet to have strong absorption effect on visible light, and the nano sheet is widely applied in the field of photocatalysis. MoS due to its strong quantum confinement effect 2 The nano-sheet can transfer electrons to TiO efficiently 2 Exhibiting excellent photocatalytic effect. Under the excitation of sunlight, photogenerated carriers are generated from MoS 2 Transfer onto the nanoplatelets to TiO 2 The photocatalysis of visible light response is realized; at the same time MoS 2 The nano-sheet loading is beneficial to the separation of electron and hole, and improves the quantum yield of photocatalysis. In addition, for TiO 2 The modification can be carried out by itself, and the visible light catalysis can be realized. The black nano titanium dioxide is prepared by using hydrogen to make part of Ti 4+ Reduction of ions to Ti 3+ The absorption spectrum of the ions is extended to the visible light region, so that the visible light response is realized. Thus, under visible light irradiation, moS 2 Nanosheet composite black TiO 2 The nano photocatalytic material can realize the high-efficiency photocatalytic sterilization functionThe effect is achieved.
Metal ions (such as silver, copper, zinc, etc.) have been used for sterilization and disinfection from ancient times. Silver is an ancient bactericide, and compared with the traditional bactericide, silver ions have higher safety, better killing effect, broad-spectrum sterilizing property and no drug resistance, and also have strong killing effect on superbacteria. However, silver ions are easy to consume by chloride ions and the like, easy to run off, easy to decompose by visible light and limited in cell absorption, which greatly limits the killing effect of the disinfectant containing silver ions; if the killing effect is achieved only by increasing the silver ion dosage, immeasurable damage is caused to human bodies and the environment, and the environment-friendly discharge standard is not met. Therefore, how to prepare safe and stable silver-containing sterilizing disinfectant has been the focus of research.
Zinc ions are an excellent mildew inhibitor but also face similar dilemmas silver ions. The nano titanium dioxide is used as an excellent carrier of metal ions, so that the stability of the ions can be enhanced, and the sterilization efficiency of the nano titanium dioxide can be enhanced; meanwhile, the addition of the metal ions also enables the nano titanium dioxide to obtain a sterilization effect under the condition of no illumination, so that the nano titanium dioxide loaded by the metal ions has a better sterilization effect than the metal ions and the nano titanium dioxide. However, due to the charge stability of the colloid, the concentration of metal ions that can be added in the nano titanium dioxide dispersion is extremely limited, and how to increase the loading of nano titanium dioxide to metal ions is extremely critical.
MoS 2 The nano material is an excellent metal ion carrier, has extremely large specific surface area and can provide a large number of adsorption sites for metal ions; s element can firmly adsorb metal ions on MoS 2 A surface. Thus, moS 2 Nanometer sheet composite black nanometer TiO 2 Is an excellent metal ionophore.
Disclosure of Invention
The primary object of the invention is to provide a black TiO with Ag/Zn ion loading 2 Composite MoS 2 The preparation method of the nano-sheet nano-material has the advantages of simple and convenient operation, easy realization, low consumption, high yield, good repeatability and suitability for mass productionPreparation of Ag/Zn ion loaded black TiO without secondary pollution to environment 2 Composite MoS 2 Nanoplatelet nanomaterials.
To achieve this object, in a basic embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 Nanoplatelets (i.e. Ag/Zn-TiO) 2 @MoS 2 ) The preparation method of the nano material comprises the following steps:
(1) Mixing molybdenum disulfide (preferably with particle size of 2-10 microns), chitosan, nano titanium dioxide (preferably commercial P25 titanium dioxide with average grain size of 20 nm) and an organic solvent to obtain a mixed solution;
(2) Ball milling is carried out on the mixed solution, and then heating and drying are carried out to obtain a powder sample;
(3) Mixing the powder sample with NaBH 4 Mixing and grinding the powder, then placing into a tubular furnace for heat treatment for a period of time, and introducing Ar gas for protection (preferably controlling the flow rate of the Ar gas to keep the tubular furnace cavity at micro positive pressure; preferably preparing TiO) 2 @MoS 2 The nano material is a heterojunction structure);
(4) Dispersing the mixed powder obtained by the heat treatment in deionized water for ultrasonic treatment, adding salt containing silver/zinc ions under stirring, and drying to obtain the nano material (preferably Ag/Zn-TiO) 2 @MoS 2 The average particle size of the nanomaterial is 100 nm).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (1), wherein the mass ratio of molybdenum disulfide to chitosan to nano-titanium dioxide is (30-75): (10-25): (0.5-2) (preferably 75:23:2).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (1), wherein in the step (1), the organic solvent is one or more selected from ethanol, glycol, NMP and DMF (preferably anhydrous ethylene glycol)Alcohols).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the step (2), wherein the ball milling treatment time is 2-6h (preferably 5 h).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (2) drying at 40-100 ℃ (preferably 80 ℃) for 2-8 hours (preferably 4 hours).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (3), wherein in the step (3), titanium dioxide and NaBH are contained in the powder sample 4 The mass ratio of the powder is 4: (0.5-1) (preferably 4:1), said grinding being carried out for a period of 20-60min (preferably 30 min).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (3) and (2) performing heat treatment at a temperature of 200-400 ℃ (preferably 300 ℃) for 0.5-3h (preferably 1 h).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (4), wherein the mass-volume ratio of titanium dioxide to deionized water in the mixed powder is 0.1-10:100 (preferably 1:100); the ultrasonic treatment is carried out for 1-4h (preferably 1 h) with power of 80-300W (preferably 240W).
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the step (4) of drying the ultrasonic treated product before adding the salt containing silver/zinc ions, wherein the temperature of the drying treatment is 40-100 ℃ and the pressure is atmospheric pressure.
In a preferred embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The preparation method of the nano-sheet nano-material comprises the following steps of (4), wherein the salt containing silver/zinc ions is silver nitrate and zinc nitrate respectively; the concentration of Ag ion after adding the salt containing silver/zinc ion is 10-1000ppm (preferably 100 ppm), and the concentration of Zn ion is 100-2000ppm (preferably 500 ppm); the stirring speed is 100-1000rpm (preferably 500 rpm) and the stirring time is 10-120min (preferably 1 h).
A second object of the present invention is to provide Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The nano-sheet nano-material has uniform size, good dispersibility, good photocatalytic effect and good sterilization effect.
To achieve this object, in a basic embodiment, the present invention provides an Ag/Zn ion-loaded black TiO 2 Composite MoS 2 The nano sheet nano material is prepared by the preparation method.
The invention has the beneficial effects that the black TiO loaded by Ag/Zn ions is utilized 2 Composite MoS 2 The nano sheet nano material and the preparation method thereof can be operated simply and conveniently, are easy to realize, have low consumption, high yield and good repeatability, are suitable for large-scale production, and have no secondary pollution to the environment for preparing Ag/Zn ion loaded black TiO 2 Composite MoS 2 The nano-sheet nano-material has uniform size, good dispersibility, good photocatalysis effect and good sterilization effect.
The beneficial effects of the invention are as follows:
1) In the invention, the black nano titanium dioxide with visible light response replaces the common P25 nano titanium dioxide excited by ultraviolet light for sterilization. In comparison, the black nano titanium dioxide can realize effective sterilization in a wider area, and has wider application prospect. In addition, in order to solve the problem of poor dispersibility of the black nano titanium dioxide, chitosan is used as a surface modifier to realize in-situ dispersion of the black nano titanium dioxide; at the same time, chitosan can also prevent the peeled disulfideThe molybdenum oxide nano-sheets are stacked again for agglomeration. Inert gas argon is used as shielding gas, which is not only favorable for reduction to obtain black nano TiO 2 And can effectively inhibit the pyrolysis of chitosan, so that the chitosan plays a role. In-situ dispersed black nano titanium dioxide is loaded on a few-layer molybdenum disulfide nanosheet, and black nano TiO is obtained 2 Composite MoS 2 Nanometer sheet (TiO) 2 @MoS 2 ) Is a composite nanomaterial of (a).
2) In the invention, ag/Zn metal ions can be adsorbed on MoS 2 The nano-sheets can be effectively adsorbed on chitosan. The chitosan not only can improve TiO 2 Visible light activity and inhibition of nano TiO 2 、MoS 2 The agglomeration of the nano-sheets can also increase the adsorption quantity of metal ions on the nano-titanium dioxide. The active groups rich in the chitosan can effectively capture free metal ions, prevent the loss of the metal ions, further promote the slow release effect of the metal ions and enhance the long-term antibacterial effect of the composite material. In addition, due to the existence of chitosan, the preparation of the powder material by direct drying is realized, and the particle size of the powder material is not increased after the powder material is redispersed. In addition, the method is simple and convenient to operate, easy to realize, short in time consumption, low in cost, high in yield, good in repeatability and suitable for large-scale production or free of secondary pollution to the environment.
3) The invention can realize the modification of the commercialized nano titanium dioxide to obtain the titanium dioxide with the visible light catalytic sterilization capability, and the silver/zinc ion loading capability is further enhanced greatly. The preparation method disclosed by the invention has large-scale industrialization capability, and expands the application of the nano titanium dioxide in the aspects of air purification, sterilization, water treatment and the like.
Drawings
FIG. 1 shows the Ag/Zn-TiO composition prepared in example 1 2 @MoS 2 Transmission electron microscopy imaging of nanomaterials.
FIG. 2 shows the Ag/Zn-TiO composition prepared in example 1 2 @MoS 2 Distribution diagram of metal element of nano material.
FIG. 3 is a schematic view ofAg/Zn-TiO prepared in example 1 2 @MoS 2 Efficiency map of photocatalytic degradation of methylene blue for nanomaterials.
FIG. 4 shows the Ag/Zn-TiO composition prepared in example 1 2 @MoS 2 A characterization diagram of the killing effect of the nano material on the escherichia coli.
Detailed Description
The following examples are presented to further illustrate embodiments of the invention. The silver nitrate, zinc nitrate, sodium borohydride, molybdenum disulfide and chitosan powders used in the examples were all purchased from ala Ding Shiji, and the P25-type nano titanium dioxide used was purchased from the winning industry group.
Example 1: ag/Zn-TiO 2 @MoS 2 Preparation of nanomaterials
(1) 3g of P25 type nano titanium dioxide powder, 0.9g of chitosan powder and 80mg of molybdenum disulfide powder are placed in an agate mortar, 5mL of absolute ethyl alcohol is added and uniformly mixed, and then the mixture is transferred into a ball milling tank for ball milling for 5 hours (500 rpm);
(2) Transferring the ball-milled sample into an oven, and drying for 4 hours at 80 ℃;
(3) The powder obtained by drying was mixed with 0.8g NaBH 4 Grinding for 30 minutes in grinding, and then transferring to a tube furnace for heat treatment at 300 ℃ for 1 hour;
(4) Dispersing the heat-treated powder in deionized water, and performing ultrasonic treatment for 1h (240W) to obtain TiO 2 The solids content of (2) is 1%;
(5) Adding a certain amount of AgNO into the dispersion liquid after ultrasonic treatment under the condition of stirring 3 And Zn (NO) 3 ) 2 The concentration of Ag ions in the dispersion was 100ppm and the concentration of Zn ions was 500ppm, and stirring was continued at normal temperature and pressure for 1 hour (500 rpm);
(6) Evaporating the obtained dispersion at 100deg.C to obtain Ag/Zn-TiO 2 @MoS 2 Nano material, namely composite nano bactericidal material powder.
Ag/Zn-TiO prepared in this example 2 @MoS 2 The nanometer material is stable and can be stored for more than 1 year at room temperature without precipitationPhenomenon. Ag/Zn-TiO obtained in this example 2 @MoS 2 The nanomaterial was characterized and the results are shown in figures 1-4. Wherein FIG. 1 is Ag/Zn-TiO 2 @MoS 2 Low power transmission electron microscopy imaging (inset) and high power transmission electron microscopy imaging (HRTEM) of the nanomaterial; FIG. 2 is an Ag/Zn-TiO 2 @MoS 2 A metal element distribution diagram of the nano material; FIG. 3 is Ag/Zn-TiO 2 @MoS 2 Nanomaterial and P25 type nano titanium dioxide and MoS 2 The comparison graph of the photocatalytic degradation dye (see GB/T23762-2020 for detection methods); FIG. 4 is an Ag/Zn-TiO 2 @MoS 2 The killing effect of the nano material on the escherichia coli under the condition of no illumination and simulated sunlight is shown (see GB/T30706-2014 for a detection method).
As can be seen from FIG. 1, ag/Zn-TiO 2 @MoS 2 TiO in nano material 2 And MoS 2 A distinct heterojunction structure is formed.
As can be seen from fig. 2, ag, mo, ti and Zn elements are simultaneously present in the prepared nanomaterial powder, i.e., the silver/zinc ion loaded titanium dioxide composite molybdenum disulfide nanomaterial is successfully prepared.
FIG. 3 compares MoS 2 Nanosheets, P25-type nano titanium dioxide and Ag/Zn-TiO 2 @MoS 2 The photocatalysis efficiency of the nano material takes methylene blue as an indicator, and under the irradiation of a light source in a sunlight simulator, tiO (titanium dioxide) 2 @MoS 2 The nanomaterial shows the strongest photocatalytic efficiency (here a nanomaterial without silver/zinc ions is used to avoid reduction of silver zinc ions to nanoparticles under photocatalysis, interfering with the photocatalytic efficiency test).
FIG. 4 is a graph comparing the concentration of Ag/Zn-TiO under dark conditions and under simulated sunlight conditions 2 @MoS 2 The killing rate of the nano material to the escherichia coli can be seen that under the irradiation of the sun, the killing rate to the escherichia coli reaches 90 percent when the concentration of the composite nano material is only 1ppm, and the composite nano material has a sterilizing effect; when the concentration is increased to 10ppm, the sterilization rate reaches 99.99 percent, and the sterilization effect is achieved.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof. The foregoing examples or embodiments are merely illustrative of the invention, which may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims are intended to be encompassed within the scope of the invention.
Claims (6)
1. Ag/Zn ion loaded black TiO 2 Composite MoS 2 The preparation method of the nano sheet nano material is characterized by comprising the following steps:
(1) Mixing molybdenum disulfide, chitosan, nano titanium dioxide and an organic solvent to obtain a mixed solution;
(2) Ball milling is carried out on the mixed solution, and then heating and drying are carried out to obtain a powder sample;
(3) Mixing the powder sample with NaBH 4 Mixing and grinding the powder, then placing the powder into a tube furnace for heat treatment for a period of time, and introducing Ar gas for protection;
(4) Dispersing the mixed powder obtained by the heat treatment in deionized water for ultrasonic treatment, adding salt containing silver/zinc ions under stirring, drying to obtain the nano material,
wherein:
in the step (1), the organic solvent is selected from one or more of ethanol, glycol, NMP and DMF;
in the step (2), the ball milling treatment time is 2-6 hours;
in the step (2), the drying temperature is 40-100 ℃ and the drying time is 2-8h.
2. According to the weightsThe method of claim 1, wherein: in the step (3), titanium dioxide and NaBH are contained in the powder sample 4 The mass ratio of the powder is 4: (0.5-1), wherein the grinding time is 20-60min.
3. The method of manufacturing according to claim 1, characterized in that: in the step (3), the temperature of the heat treatment is 200-400 ℃ and the time is 0.5-3h.
4. The method of manufacturing according to claim 1, characterized in that: in the step (4), the mass-volume ratio of the titanium dioxide to the deionized water in the mixed powder is 0.1-10:100; the ultrasonic treatment time is 1-4h, and the power is 80-300W.
5. The method of manufacturing according to claim 1, characterized in that: in the step (4), the salts containing silver/zinc ions are silver nitrate and zinc nitrate respectively; the concentration of Ag ions is 10-1000ppm and the concentration of Zn ions is 100-2000ppm after adding the salt containing silver/zinc ions; the stirring speed is 100-1000rpm, and the stirring time is 10-120min.
6. Ag/Zn ion loaded black TiO 2 Composite MoS 2 The nano sheet nano material is characterized in that: the nanomaterial is prepared by the preparation method according to any one of claims 1 to 5.
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